CN113597447A - Insulating resin composition and method for producing same, insulating tape and method for producing same, method for forming insulating layer, and power cable and method for producing same - Google Patents
Insulating resin composition and method for producing same, insulating tape and method for producing same, method for forming insulating layer, and power cable and method for producing same Download PDFInfo
- Publication number
- CN113597447A CN113597447A CN202080022409.7A CN202080022409A CN113597447A CN 113597447 A CN113597447 A CN 113597447A CN 202080022409 A CN202080022409 A CN 202080022409A CN 113597447 A CN113597447 A CN 113597447A
- Authority
- CN
- China
- Prior art keywords
- insulating
- resin
- polyolefin resin
- insulating layer
- resin composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000011342 resin composition Substances 0.000 title claims abstract description 145
- 238000000034 method Methods 0.000 title claims description 82
- 238000004519 manufacturing process Methods 0.000 title claims description 41
- 229920005672 polyolefin resin Polymers 0.000 claims abstract description 181
- 229920005989 resin Polymers 0.000 claims abstract description 151
- 239000011347 resin Substances 0.000 claims abstract description 151
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 46
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 44
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 28
- 150000001990 dicarboxylic acid derivatives Chemical class 0.000 claims abstract description 16
- 239000004020 conductor Substances 0.000 claims description 58
- 238000004132 cross linking Methods 0.000 claims description 48
- 239000003431 cross linking reagent Substances 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 31
- 238000002844 melting Methods 0.000 claims description 29
- 230000008018 melting Effects 0.000 claims description 29
- 239000002994 raw material Substances 0.000 claims description 27
- 238000001125 extrusion Methods 0.000 claims description 25
- 239000008188 pellet Substances 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 238000004804 winding Methods 0.000 claims description 14
- 229920000098 polyolefin Polymers 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 238000010030 laminating Methods 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 abstract description 16
- 238000004898 kneading Methods 0.000 description 36
- 238000011156 evaluation Methods 0.000 description 31
- -1 polyethylene chain Polymers 0.000 description 27
- 230000005684 electric field Effects 0.000 description 20
- 229910052751 metal Inorganic materials 0.000 description 16
- 239000002184 metal Substances 0.000 description 16
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 14
- 239000004698 Polyethylene Substances 0.000 description 13
- 229920000573 polyethylene Polymers 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000012321 sodium triacetoxyborohydride Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 239000004743 Polypropylene Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 9
- 230000005484 gravity Effects 0.000 description 9
- 229920001684 low density polyethylene Polymers 0.000 description 8
- 239000004702 low-density polyethylene Substances 0.000 description 8
- 229920001155 polypropylene Polymers 0.000 description 8
- 230000002159 abnormal effect Effects 0.000 description 7
- 238000009825 accumulation Methods 0.000 description 7
- 229920013716 polyethylene resin Polymers 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 239000011256 inorganic filler Substances 0.000 description 5
- 229910003475 inorganic filler Inorganic materials 0.000 description 5
- 238000005979 thermal decomposition reaction Methods 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 3
- 229920001912 maleic anhydride grafted polyethylene Polymers 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- HXIQYSLFEXIOAV-UHFFFAOYSA-N 2-tert-butyl-4-(5-tert-butyl-4-hydroxy-2-methylphenyl)sulfanyl-5-methylphenol Chemical compound CC1=CC(O)=C(C(C)(C)C)C=C1SC1=CC(C(C)(C)C)=C(O)C=C1C HXIQYSLFEXIOAV-UHFFFAOYSA-N 0.000 description 2
- PFANXOISJYKQRP-UHFFFAOYSA-N 2-tert-butyl-4-[1-(5-tert-butyl-4-hydroxy-2-methylphenyl)butyl]-5-methylphenol Chemical compound C=1C(C(C)(C)C)=C(O)C=C(C)C=1C(CCC)C1=CC(C(C)(C)C)=C(O)C=C1C PFANXOISJYKQRP-UHFFFAOYSA-N 0.000 description 2
- VSAWBBYYMBQKIK-UHFFFAOYSA-N 4-[[3,5-bis[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-2,4,6-trimethylphenyl]methyl]-2,6-ditert-butylphenol Chemical compound CC1=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C1CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 VSAWBBYYMBQKIK-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- CGRTZESQZZGAAU-UHFFFAOYSA-N [2-[3-[1-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoyloxy]-2-methylpropan-2-yl]-2,4,8,10-tetraoxaspiro[5.5]undecan-9-yl]-2-methylpropyl] 3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C)=CC(CCC(=O)OCC(C)(C)C2OCC3(CO2)COC(OC3)C(C)(C)COC(=O)CCC=2C=C(C(O)=C(C)C=2)C(C)(C)C)=C1 CGRTZESQZZGAAU-UHFFFAOYSA-N 0.000 description 2
- BEIOEBMXPVYLRY-UHFFFAOYSA-N [4-[4-bis(2,4-ditert-butylphenoxy)phosphanylphenyl]phenyl]-bis(2,4-ditert-butylphenoxy)phosphane Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(C=1C=CC(=CC=1)C=1C=CC(=CC=1)P(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C BEIOEBMXPVYLRY-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 229920003020 cross-linked polyethylene Polymers 0.000 description 2
- 239000004703 cross-linked polyethylene Substances 0.000 description 2
- 150000001991 dicarboxylic acids Chemical class 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229920005648 ethylene methacrylic acid copolymer Polymers 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- NKHAVTQWNUWKEO-UHFFFAOYSA-N fumaric acid monomethyl ester Natural products COC(=O)C=CC(O)=O NKHAVTQWNUWKEO-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- GWWYBYNZFWRRSG-UHFFFAOYSA-N hydroxyphosphanyloxyphosphinous acid;1,2,3,4-tetrakis(2,4-ditert-butylphenyl)biphenylene Chemical compound OPOPO.CC(C)(C)C1=CC(C(C)(C)C)=CC=C1C(C(=C1C=2C(=CC(=CC=2)C(C)(C)C)C(C)(C)C)C=2C(=CC(=CC=2)C(C)(C)C)C(C)(C)C)=C(C=2C3=CC=CC=2)C3=C1C1=CC=C(C(C)(C)C)C=C1C(C)(C)C GWWYBYNZFWRRSG-UHFFFAOYSA-N 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 2
- 150000001451 organic peroxides Chemical class 0.000 description 2
- 239000002530 phenolic antioxidant Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 239000012756 surface treatment agent Substances 0.000 description 2
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
- JHVQEUGNYSVSDH-UHFFFAOYSA-N (4-methylnaphthalen-1-yl)boronic acid Chemical compound C1=CC=C2C(C)=CC=C(B(O)O)C2=C1 JHVQEUGNYSVSDH-UHFFFAOYSA-N 0.000 description 1
- VNQNXQYZMPJLQX-UHFFFAOYSA-N 1,3,5-tris[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-1,3,5-triazinane-2,4,6-trione Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CN2C(N(CC=3C=C(C(O)=C(C=3)C(C)(C)C)C(C)(C)C)C(=O)N(CC=3C=C(C(O)=C(C=3)C(C)(C)C)C(C)(C)C)C2=O)=O)=C1 VNQNXQYZMPJLQX-UHFFFAOYSA-N 0.000 description 1
- BQTPKSBXMONSJI-UHFFFAOYSA-N 1-cyclohexylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1CCCCC1 BQTPKSBXMONSJI-UHFFFAOYSA-N 0.000 description 1
- HIDBROSJWZYGSZ-UHFFFAOYSA-N 1-phenylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC=C1 HIDBROSJWZYGSZ-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 description 1
- GJDRKHHGPHLVNI-UHFFFAOYSA-N 2,6-ditert-butyl-4-(diethoxyphosphorylmethyl)phenol Chemical compound CCOP(=O)(OCC)CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 GJDRKHHGPHLVNI-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- QSRJVOOOWGXUDY-UHFFFAOYSA-N 2-[2-[2-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoyloxy]ethoxy]ethoxy]ethyl 3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C)=CC(CCC(=O)OCCOCCOCCOC(=O)CCC=2C=C(C(O)=C(C)C=2)C(C)(C)C)=C1 QSRJVOOOWGXUDY-UHFFFAOYSA-N 0.000 description 1
- VFBJXXJYHWLXRM-UHFFFAOYSA-N 2-[2-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]ethylsulfanyl]ethyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCCSCCOC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 VFBJXXJYHWLXRM-UHFFFAOYSA-N 0.000 description 1
- GAODDBNJCKQQDY-UHFFFAOYSA-N 2-methyl-4,6-bis(octylsulfanylmethyl)phenol Chemical compound CCCCCCCCSCC1=CC(C)=C(O)C(CSCCCCCCCC)=C1 GAODDBNJCKQQDY-UHFFFAOYSA-N 0.000 description 1
- AIBRSVLEQRWAEG-UHFFFAOYSA-N 3,9-bis(2,4-ditert-butylphenoxy)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP1OCC2(COP(OC=3C(=CC(=CC=3)C(C)(C)C)C(C)(C)C)OC2)CO1 AIBRSVLEQRWAEG-UHFFFAOYSA-N 0.000 description 1
- SSADPHQCUURWSW-UHFFFAOYSA-N 3,9-bis(2,6-ditert-butyl-4-methylphenoxy)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound CC(C)(C)C1=CC(C)=CC(C(C)(C)C)=C1OP1OCC2(COP(OC=3C(=CC(C)=CC=3C(C)(C)C)C(C)(C)C)OC2)CO1 SSADPHQCUURWSW-UHFFFAOYSA-N 0.000 description 1
- OFNISBHGPNMTMS-UHFFFAOYSA-N 3-methylideneoxolane-2,5-dione Chemical compound C=C1CC(=O)OC1=O OFNISBHGPNMTMS-UHFFFAOYSA-N 0.000 description 1
- QRLSTWVLSWCGBT-UHFFFAOYSA-N 4-((4,6-bis(octylthio)-1,3,5-triazin-2-yl)amino)-2,6-di-tert-butylphenol Chemical compound CCCCCCCCSC1=NC(SCCCCCCCC)=NC(NC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=N1 QRLSTWVLSWCGBT-UHFFFAOYSA-N 0.000 description 1
- BHQCQFFYRZLCQQ-UHFFFAOYSA-N 4-(3,7,12-trihydroxy-10,13-dimethyl-2,3,4,5,6,7,8,9,11,12,14,15,16,17-tetradecahydro-1h-cyclopenta[a]phenanthren-17-yl)pentanoic acid Chemical compound OC1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(O)=O)C)C1(C)C(O)C2 BHQCQFFYRZLCQQ-UHFFFAOYSA-N 0.000 description 1
- ZVVFVKJZNVSANF-UHFFFAOYSA-N 6-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]hexyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCCCCCCOC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 ZVVFVKJZNVSANF-UHFFFAOYSA-N 0.000 description 1
- ADRNSOYXKABLGT-UHFFFAOYSA-N 8-methylnonyl diphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OCCCCCCCC(C)C)OC1=CC=CC=C1 ADRNSOYXKABLGT-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- IEPRKVQEAMIZSS-UHFFFAOYSA-N Di-Et ester-Fumaric acid Natural products CCOC(=O)C=CC(=O)OCC IEPRKVQEAMIZSS-UHFFFAOYSA-N 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- IEPRKVQEAMIZSS-WAYWQWQTSA-N Diethyl maleate Chemical compound CCOC(=O)\C=C/C(=O)OCC IEPRKVQEAMIZSS-WAYWQWQTSA-N 0.000 description 1
- XLYMOEINVGRTEX-ARJAWSKDSA-N Ethyl hydrogen fumarate Chemical compound CCOC(=O)\C=C/C(O)=O XLYMOEINVGRTEX-ARJAWSKDSA-N 0.000 description 1
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 description 1
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 229920003354 Modic® Polymers 0.000 description 1
- 229920003298 Nucrel® Polymers 0.000 description 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- QWEDYNXINZOSSV-AATRIKPKSA-N [2-methyl-4-oxo-3-[(e)-prop-1-enyl]cyclopent-2-en-1-yl] n,n-dimethylcarbamate Chemical compound C\C=C\C1=C(C)C(OC(=O)N(C)C)CC1=O QWEDYNXINZOSSV-AATRIKPKSA-N 0.000 description 1
- IORUEKDKNHHQAL-UHFFFAOYSA-N [2-tert-butyl-6-[(3-tert-butyl-2-hydroxy-5-methylphenyl)methyl]-4-methylphenyl] prop-2-enoate Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)OC(=O)C=C)=C1O IORUEKDKNHHQAL-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H02G1/00—Methods or apparatus specially adapted for installing, maintaining, repairing or dismantling electric cables or lines
- H02G1/14—Methods or apparatus specially adapted for installing, maintaining, repairing or dismantling electric cables or lines for joining or terminating cables
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
The invention provides an insulating resin composition which is less in the amount of space charge accumulated in an insulating layer and thus less likely to cause dielectric breakdown. The insulating resin composition 1 comprises at least a base resin and an antioxidant, wherein the base resin contains a modified polyolefin resin modified with a molecule having a polar group and an unmodified polyolefin resin, the modified polyolefin resin is modified with at least 1 selected from an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative as a molecule having a polar group, the base resin has a so-called sea-island structure in which a second phase 12 containing the modified polyolefin resin is present in a first phase 11 containing the unmodified polyolefin resin, and the second phase has an average diameter of 2 [ mu ] m or less.
Description
Technical Field
The present invention relates to an insulating resin composition and a method for producing the insulating resin composition, an insulating tape formed using the insulating resin composition and used for coating a connection portion of a power cable, a method for producing the insulating tape, a method for forming an insulating layer on an outer surface of a connection portion of a power cable using the insulating tape, and a power cable having an insulating layer formed using the insulating resin composition and a method for producing the power cable.
Background
As a power transmission and distribution cable (power cable) for electric power, a cable having a conductor and an insulating layer covering the outer periphery of the conductor and containing a crosslinked polyolefin resin such as a crosslinked polyethylene resin is widely used. However, it is known that a crosslinked polyolefin resin constituting an insulating layer of a power cable is easily damaged by deterioration due to accumulation of space charges therein with the passage of time. Therefore, in the power cable, it is preferable to reduce the amount of space charge accumulated in the insulating layer so as not to cause dielectric breakdown.
As a means for reducing the amount of space charge accumulated in the insulating layer, there is a method of modifying a polyolefin resin constituting the insulating layer. More specifically, there may be mentioned: a method of adding an electric field stabilizer, a dendronization-resistant additive, etc. to a polyolefin resin; a method of blending 2 or more polymers; and a method of developing a new material by grafting a monomer having an appropriate polar group to a polyethylene chain or modifying a polymerization process to copolymerize it with other polymers; and the like (see, for example, non-patent document 1).
Among these, as a method for adding an electric field stabilizer, a dendrite resistance additive, and the like to a polyolefin, for example, patent document 1 describes a cable in which a polar inorganic filler obtained by performing surface treatment with a surface treatment agent and pulverizing the surface treatment agent to have a particle diameter substantially equal to that of the polar inorganic filler before the surface treatment is used as the polar inorganic filler in a direct current cable having an insulating layer made of crosslinked polyethylene containing the polar inorganic filler such as magnesium oxide. Further, by adding magnesium oxide, the decrease in volume resistivity and the accumulation of space charge due to the decomposition residue of an organic peroxide crosslinking agent such as DCP (dicumyl peroxide) are suppressed, and the dc insulation characteristics of the insulating layer are improved.
In addition, as a method of grafting a monomer having an appropriate polar group to a polyethylene chain, for example, patent document 2 describes an alternating current power cable having a density of 0.93g/cm3The maleic anhydride-grafted polyethylene having a maleic anhydride concentration of 0.01 to 5 wt% is used for an insulator. Further, by diluting the maleic anhydride-grafted polyethylene with polyethylene, an appropriate amount of carbonyl groups are added to the resin of the insulator, and the added carbonyl groups act as a space charge trap, whereby the movement of space charges can be suppressed, and therefore, the occurrence of dc dielectric breakdown due to the accumulation of local space charges is suppressed.
Documents of the prior art
Patent document
Patent document 1: japanese laid-open patent publication No. 11-086634
Patent document 2: japanese laid-open patent publication No. 2004-363020
Non-patent document
Non-patent document 1: li Changlong, two other people, journal of the institute of Electrical and electronics treatise A (journal of Foundation, Material, department of Community), Vol.118, No. 10, 1998, p.1094-1100
Disclosure of Invention
Problems to be solved by the invention
In the direct current cable described in patent document 1, since an inorganic filler having a higher specific gravity than the resin is added to the resin of the insulating layer, there are problems that the cable becomes heavy and workability in using the cable is poor, and that insulation breakdown is easily caused by mixing of large filler particles of 100 μm or more.
In addition, in the ac power cable described in patent document 2, if kneading of the resin is insufficient when the maleic anhydride-grafted polyethylene is diluted, there is a problem as follows: the distribution of polar groups in the resin composition becomes uneven, and the amount of space charge accumulated in the insulating layer varies, and dielectric breakdown is likely to occur in a portion having a small carbonyl group. On the other hand, if the temperature of the resin during kneading is increased or the rotational speed of the screw of the extruder is increased for the purpose of improving the uniformity, there is a problem that abnormal crosslinking of the resin occurs due to shear heat, and molding becomes difficult.
The object of the present invention is to provide: an insulating resin composition which has a small amount of space charge accumulated in an insulating layer and is less likely to cause dielectric breakdown, and a method for producing the same; an insulating tape formed using the insulating resin composition and usable for coating a connection portion of a power cable, and a method for producing the same; a method for forming an insulating layer on the outer surface of a connection portion of a power cable using the insulating tape; and a power cable having an insulating layer formed using the insulating resin composition and a method for manufacturing the same.
Means for solving the problems
As a result of intensive studies, the inventors of the present application have found that, when a modified polyolefin modified with a molecule having a polar group is used for an insulating layer of a power cable, it is more effective in reducing the amount of space charge accumulated in the insulating layer to form a so-called sea-island structure in which a second phase containing a modified polyolefin resin is present in a first phase containing an unmodified polyolefin resin, and have completed the present invention based on such findings.
That is, the gist of the present invention is as follows.
(1) An insulating resin composition comprising at least a base resin and an antioxidant, wherein the base resin comprises a modified polyolefin resin modified with a molecule having a polar group and an unmodified polyolefin resin, the modified polyolefin resin is modified with at least 1 selected from the group consisting of an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative as a molecule having a polar group, the base resin has a so-called sea-island structure in which a second phase comprising the modified polyolefin resin is present in a first phase comprising the unmodified polyolefin resin, and the second phase has an average diameter of 2 [ mu ] m or less.
(2) An insulating tape for forming an insulating layer of a power cable, which is produced from the insulating resin composition as described in (1) above, and which has a tape thickness in the range of 30 to 250 μm and a tape width in the range of 3 to 40 mm.
(3) A power cable having a conductor; and a composite coating film formed by laminating an inner semiconductive layer made of a first conductive resin, an insulating layer, and an outer semiconductive layer made of a second conductive resin in this order on the outer periphery of the conductor, wherein the insulating layer is formed by using the insulating resin composition described in the above (1) as a raw material and crosslinking at least the modified polyolefin resin in the second phase and at least the unmodified polyolefin resin in the first phase.
(4) A power cable including a connection structure portion, the connection structure portion including: a connecting section in which the exposed ends of the conductors of the plurality of power cables are conductor-connected to each other; and a composite coating film formed by laminating an inner semiconductive layer made of a first conductive resin, an insulating layer, and an outer semiconductive layer made of a second conductive resin in this order on the outer periphery of the connecting portion, wherein the insulating layer is formed by using the insulating resin composition described in (1) above as a raw material and crosslinking at least the modified polyolefin resin in the second phase and at least the unmodified polyolefin resin in the first phase.
(5) The power cable according to (4) above, wherein the insulating layer is formed by winding and crosslinking an insulating tape for forming an insulating layer having a tape thickness in a range of 30 μm or more and 250 μm or less and a tape width in a range of 3mm or more and 40mm or less around the outer periphery of the inner semiconductive layer.
(6) The power cable according to any one of the above (3) to (5), wherein a total thickness of the inner semiconductive layer and the outer semiconductive layer is 5mm or less.
(7) A method for producing an insulating resin composition, comprising the steps of: an unmodified polyolefin resin and an antioxidant are added to a modified polyolefin resin modified with at least 1 selected from an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative which are molecules having a polar group, and then kneaded to obtain a base resin in which the modified polyolefin resin is diluted with the unmodified polyolefin resin, wherein the base resin has a so-called sea-island structure in which a second phase containing the modified polyolefin resin is present in a first phase containing the unmodified polyolefin resin, and the second phase has an average diameter of 2 [ mu ] m or less.
(8) A method for producing an insulating resin composition, comprising the steps of: a method for producing a polyolefin resin composition, which comprises adding an unmodified polyolefin resin and an antioxidant to a modified polyolefin resin modified with at least 1 selected from an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative which are molecules having a polar group, to prepare a diluted polyolefin pellet comprising a base resin in which the modified polyolefin resin is diluted with the unmodified polyolefin resin, adding a crosslinking agent to the prepared diluted polyolefin pellet, and dry-blending the pellets so that the base resin has a so-called sea-island structure in which a second phase comprising the modified polyolefin resin is present in a first phase comprising the unmodified polyolefin resin and the average diameter of the second phase is 2 [ mu ] m or less.
(9) A method for manufacturing an insulating tape for forming an insulating layer of a power cable, the method comprising: a step of forming a film by extrusion molding the insulating resin composition of (1) above, and cooling the surface temperature of the film to the melting point of the unmodified polyolefin resin or less within 15 seconds after the insulating resin composition is extruded; and a step of slitting the film to form a tape.
(10) A method for forming an insulating layer on the outer surface of a connecting portion of a power cable, comprising the steps of: forming an insulating layer on an outer surface of a connecting part by using the insulating resin composition according to the above (1) on an outer periphery of the connecting part in which exposed ends of conductors of a plurality of power cables are conductor-connected to each other, and subjecting the connecting part on which the insulating layer is formed to a pressure-heating treatment under conditions of 300kPa or more and 1000kPa or less and 140 ℃ or more and 280 ℃ or less to crosslink an unmodified polyolefin resin and a modified polyolefin resin of the base resin included in the insulating layer.
(11) The method for forming an insulating layer according to item (10) above, wherein the insulating layer is formed on the outer periphery of the connecting portion by winding an insulating tape for forming an insulating layer, the insulating tape being made of the insulating resin composition, having a tape thickness in a range of 30 μm to 250 μm, and having a tape width in a range of 3mm to 40 mm.
(12) A method for manufacturing a power cable, comprising the steps of sequentially laminating an inner semiconductive layer, an insulating layer and an outer semiconductive layer on the outer periphery of a conductor, and crosslinking at least the insulating layer, wherein the laminating of the insulating layer is performed by extruding the insulating resin composition according to the above (1) onto the outer periphery of the inner semiconductive layer, and the surface temperature of the laminated insulating layer is cooled to the melting point of the unmodified polyolefin resin or less within 15 seconds after the extruding onto the outer periphery of the inner semiconductive layer, and the crosslinking step of the insulating layer is performed by: and subjecting the insulating layer to a pressure-heating treatment under conditions of 300kPa to 1000kPa inclusive and 140 ℃ to 280 ℃ inclusive, thereby crosslinking the unmodified polyolefin resin and the modified polyolefin resin of the base resin contained in the insulating layer.
ADVANTAGEOUS EFFECTS OF INVENTION
According to the present invention, since the insulating resin composition has a so-called sea-island structure in which the second phase (island phase) containing the modified polyolefin resin is present in the first phase (sea phase) containing the unmodified polyolefin resin and the size of the second phase (island phase) is as small as 2 μm or less, the unevenness in the distribution of the polar groups is reduced, and therefore, the amount of space charge accumulated in the insulating resin composition can be reduced. Thus, an insulating resin composition which is less likely to cause dielectric breakdown, a method for producing the same, an insulating tape formed using the insulating resin composition, a method for producing the same, a method for forming an insulating layer using the insulating tape, a power cable using the insulating resin composition, and a method for producing the same can be obtained.
Drawings
FIG. 1 is a schematic view illustrating a sea-island structure of an insulating resin composition according to the present invention.
Fig. 2 is a diagram illustrating a power cable according to the present invention. Fig. 2(a) is a cross-sectional view schematically showing the power cable. Fig. 2(b) is a cross-sectional view taken along line a-a' of fig. 2 (a).
Fig. 3 is a diagram illustrating a power cable having a connection structure portion formed by winding an insulating tape according to the present invention. Fig. 3(a) is a schematic cross-sectional view of a power cable including a connection structure portion. Fig. 3(B) is a cross-sectional view taken along line B-B' of fig. 3 (a). Further, FIG. 3(C) is a sectional view taken along line C-C' of FIG. 3 (a).
Fig. 4 is a diagram illustrating a method for forming an insulating layer on an outer surface of a connection portion of a power cable according to the present invention. Fig. 4(a) is a cross-sectional view showing the end portions of 2 power cables with the conductors at the end portions exposed, in a separated state facing each other. Fig. 4(b) is a cross-sectional view showing a state in which the exposed end portions of the conductors are connected to each other by the conductors. Fig. 4(c) is a cross-sectional view showing a state in which an inner semiconductive layer is formed on the outer periphery of the connection portion. Fig. 4(d) is a cross-sectional view showing a state in which an insulating layer is formed on the outer periphery of the inner semiconductive layer of the connection portion. Fig. 4(e) is a cross-sectional view showing a state in which an outer semiconductive layer is formed on the outer periphery of an insulating layer.
Fig. 5 is a front view showing an example (example) of a screw having a resin mixing portion provided at a tip portion of a full-flight screw, which is suitably used for extrusion molding in the method for producing an insulating resin composition according to the present invention.
Fig. 6 is a front view showing an example of a screw having a general full-flight screw used for extrusion molding in the method for producing an insulating resin composition.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail. The present invention is not limited to the following embodiments, and various modifications can be made without departing from the scope of the present invention.
< insulating resin composition >
The insulating resin composition of the present invention comprises at least a base resin and an antioxidant, wherein the base resin contains a modified polyolefin resin modified with a molecule having a polar group and an unmodified polyolefin resin. Here, the modified polyolefin resin is formed by modifying at least 1 kind selected from the group consisting of an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride, and an unsaturated dicarboxylic anhydride derivative, which are molecules having a polar group. In addition, the base resin has a so-called sea-island structure in which a second phase comprising a modified polyolefin resin is present in a first phase comprising an unmodified polyolefin resin, and the second phase has an average diameter of 2 μm or less.
The insulating resin composition according to the present embodiment has a so-called sea-island structure in which the second phase (island phase) containing the modified polyolefin resin is present in the first phase (sea phase) containing the modified polyolefin resin, and the second phase (island phase) is made fine so that the size is 2 μm or less, whereby the unevenness in the distribution of the polar groups is reduced, and therefore, the amount of space charge accumulated in the insulating layer can be effectively reduced, and as a result, dielectric breakdown in the insulating layer can be made less likely to occur.
The insulating resin composition according to the present embodiment contains at least a base resin (a) and an antioxidant (C). The insulating resin composition according to the present embodiment preferably further contains a crosslinking agent (B).
[ base resin (A) ]
The base resin (a) is composed of a modified polyolefin resin (a1) modified with a molecule having a polar group and an unmodified polyolefin resin (a 2). Thus, in the insulating resin composition, the modified polyolefin resin (a1) having high hydrophilicity and the unmodified polyolefin resin (a2) having high hydrophobicity coexist, and therefore, a so-called sea-island structure in which the second phase including the modified polyolefin resin (a1) is present in the first phase including the unmodified polyolefin resin (a2) can be formed.
Here, the "sea-island structure" is, for example, a structure shown in fig. 1 in which a second phase 12 called an island phase exists in a first phase 11 called a sea phase. Therefore, in the insulating resin composition 1 according to the present embodiment, the second phase (island phase) 12 containing the modified polyolefin resin (a1) is present in the first phase (sea phase) 11 containing the unmodified polyolefin resin (a 2). With such a configuration, the accumulation of space charges when a current is passed through the power cable can be reduced, and therefore, dielectric breakdown can be reduced in the insulating layer formed of the insulating resin composition 1.
Here, the average diameter of the second phase (island phase) 12 in the sea-island structure is 2 μm or less. Accordingly, even when a current is passed through the power cable, the accumulation of space charges in the island phase is less likely to occur, and therefore, the insulating layer formed of the insulating resin composition 1 can suppress the reduction in insulating performance due to local electric field concentration.
In addition, it is preferable that the second phases (island phases) 12 in the sea-island structure are present in a range of 5 to 20 second phases (island phases) having a diameter in a range of 0.5 to 2.0 μm in an observation range of 10 μm in the vertical direction × 10 μm in the horizontal direction, and the sum of the areas of all the second phases (island phases) 12 is 20 μm2The following. Thus, the distribution of the polar groups in the insulating resin composition is further variedTherefore, the accumulation of space charge is also dispersed, whereby dielectric breakdown in the insulating layer can be made less likely to occur.
The confirmation of the insulating resin composition having a sea-island structure, the measurement of the diameter of the second phase (island phase) contained in the sea-island structure, and the measurement of the number of second phases (island phases) having a diameter in the range of 0.5 to 2 μm can be carried out by: after the metal staining is performed as necessary, the resin composition and a cross section thereof are observed using, for example, a Transmission Electron Microscope (TEM). Here, the average diameter of the island phase was measured by: the transmission electron microscope was set to a magnification of 10000 times, and the average diameter of the islands taken was determined using 1 image taken by adjusting the contrast so that the island structure could be identified. Here, the diameter of the second phase (island phase) is obtained by using image processing, and the maximum value and the minimum value when the size of the island phase is measured over the entire circumference (360 degrees) are respectively set as the maximum size and the minimum size, and the arithmetic average of these maximum size and minimum size is obtained.
(modified polyolefin resin (A1))
As the modified polyolefin resin (a1) contained in the base resin (a), a modified polyolefin resin modified with a molecule having a polar group is used. The modified polyolefin resin (A1) is contained in the second phase (island phase) of the sea-island structure.
The modified polyolefin resin (a1) is a polyolefin resin modified by bonding molecules having polar groups.
Here, the polyolefin resin is preferably a polyethylene resin, a polypropylene resin, or a copolymer thereof. The modified polyolefin resin (a1) must be modified with at least 1 selected from the group consisting of unsaturated dicarboxylic acids, unsaturated dicarboxylic anhydrides, and derivatives of unsaturated dicarboxylic acids, which are molecules having polar groups.
Examples of the unsaturated dicarboxylic acid in the molecule having a polar group include maleic acid, fumaric acid, and itaconic acid. Examples of the unsaturated dicarboxylic anhydride include maleic anhydride and itaconic anhydride. Examples of the derivative of the unsaturated dicarboxylic acid include monomethyl ester, monoethyl ester, diethyl ester, amide, and imide of the unsaturated dicarboxylic acid. More specifically, monomethyl maleate, monoethyl maleate, diethyl maleate, monomethyl fumarate, dimethyl fumarate, diethyl fumarate, monoamide maleate, maleimide, N-methylmaleimide, N-phenylmaleimide, and N-cyclohexylmaleimide can be mentioned. Among these, maleic anhydride having the highest ratio of carbonyl groups per unit molecular weight is most preferably used in order to impart hydrophilicity to the polyolefin resin by adding a small amount. These molecules having a polar group may be used alone or in combination of 2 or more.
As the modified polyolefin resin (a1), a commercially available resin can be used in addition to the modified polyolefin resin obtained by modifying a polyolefin resin with a molecule having a polar group as described above. For example, HIMILAN (ionomer resin, Dupont-Mitsui Polychemical Co., Ltd.), NUCREL (ethylene-methacrylic acid copolymer, Dupont Kabushiki Kaisha), SCONA TSPE (maleic anhydride-modified low-density polyethylene, BYK Kaisha), OREVACG (maleic anhydride-modified low-density polyethylene, Arkema Kaisha), MODIC (maleic anhydride-modified low-density polyethylene, Mitsubishi chemical), Youmex (maleic anhydride-modified polypropylene, Sanyo Kasei Kaisha), REO-070-1 (maleic anhydride-modified polypropylene, RikenVitami Co., Ltd.), Kayabrid (maleic anhydride-modified polypropylene, Kayakuzo), SCONTPA PP (maleic anhydride-modified low-density polyethylene, BYK Kaisha), ADMER (maleic anhydride-modified polypropylene, Mitsui chemical Co., Ltd.), and the like can be suitably used.
The melting point of the modified polyolefin resin (A1) is preferably 90 ℃ or higher and 140 ℃ or lower, more preferably 90 ℃ or higher and 130 ℃ or lower, and still more preferably 100 ℃ or higher and 120 ℃ or lower in the measurement by differential scanning calorimetry of JIS K7121-1987.
(unmodified polyolefin resin (A2))
The unmodified polyolefin resin (a2) contained in the base resin (a) is contained in the first phase (sea phase) of the sea-island structure, and functions as a dispersion medium for the modified polyolefin resin (a 1).
As the unmodified polyolefin resin (a2), known unmodified polyolefin resins can be used, and among them, low-density polyethylene as polyethylene having a branched structure, polypropylene, and a copolymer of linear low-density polyethylene and an olefin, which has a specific gravity of 0.900 to 0.940, are preferably contained. This improves flexibility when the insulating tape or the insulating layer is formed from the insulating resin composition, and thus, handling of the power cable can be facilitated.
The melting point of the unmodified polyolefin resin (A2) is preferably 90 ℃ to 170 ℃, preferably 90 ℃ to 130 ℃, and more preferably 100 ℃ to 120 ℃ in the measurement by differential scanning calorimetry of JIS K7121-1987.
The ratio of the modified polyolefin resin (a1) and the unmodified polyolefin resin (a2) constituting the base resin (a) is preferably 2 parts by mass or more and 20 parts by mass or less of the unmodified polyolefin resin (a2) to 1 part by mass of the modified polyolefin resin (a1) from the viewpoint of facilitating the kneading with an additive and obtaining a uniform resin and from the viewpoint of appropriately adjusting the concentration of hydrophilic groups.
[ crosslinking agent (B) ]
In the resin composition of the present invention, it is preferable to add a crosslinking agent (B) in order to crosslink the base resin (a). The crosslinking agent (B) improves the mechanical properties and heat resistance of the resin material by crosslinking the base resin (a), and also has a function of bonding adjacent insulating tapes when an insulating layer is formed using an insulating tape containing an insulating resin composition.
The crosslinking agent (B) preferably contains an organic peroxide which generates a radical by thermal decomposition during heating.
Specific examples of the crosslinking agent (B) include dicumyl peroxide (DCP), benzoyl peroxide, benzoyl dichloride peroxide, di-t-butyl peroxide, butyl peroxyacetate, t-butyl peroxybenzoate, 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, and the like. Among them, DCP is preferably contained. Further, 2 or more of these compounds may be contained in combination as the crosslinking agent (B).
The lower limit of the content of the crosslinking agent (B) is preferably 0.1 part by mass or more, and more preferably 0.5 part by mass or more, based on 100 parts by mass of the total of the base resins (a). Thus, the mechanical properties and heat resistance of the resin material can be improved by crosslinking the polyolefin resin. On the other hand, the upper limit of the content of the crosslinking agent (B) is preferably 5 parts by mass, more preferably 3 parts by mass, based on 100 parts by mass of the total of the base resins (a). This can suppress a decrease in electrical characteristics due to abnormal crosslinking when the insulating resin composition is extrusion-molded.
[ antioxidant (C) ]
The antioxidant (C) is also called an antioxidant, and has an effect of preventing the insulating resin composition, the insulating tape formed of the insulating resin composition, and the insulating layer from being deteriorated by heat or oxygen in the air.
The antioxidant (C) includes 1 or more antioxidants selected from the group consisting of phenol-based, phosphorus-based, sulfur-based, amine-based, hydrazine-based and amide-based antioxidants, and derivatives thereof. In particular, 2 or more of these compounds may be used in combination as the antioxidant (C). The antioxidant (C) preferably contains a phenol-based antioxidant or an amine-based antioxidant, and a phosphoric acid-based antioxidant or a sulfur-based antioxidant.
Specific examples of the phenolic antioxidant include IRGANOX 245, IRGANOX 259, IRGANOX 565, IRGANOX1010, IRGANOX 1035, IRGANOX 1076, IRGANOX 1098, IRGANOX 1222, IRGANOX 1330, IRGANOX 1425, IRGANOX 3114, IRGANOX 1520, IRGANOX 1135, IRGANOX 1141 (all of which are manufactured by BASF Co., Ltd.), Sumilizer BHT, Sumilizer MDP-S, Sumilizer GA-80, Sumilizer BBM-S, Sumilizer WX-R, Sumilizer GM (all of which are manufactured by Sumitomo chemical Co., Ltd.), ADK STAB-20, ADSTAK B AO-30, ADSTAK STAB AO-40, ADK STAB AO-50, ADK STAB AO-80, and ADK STAB-330 (manufactured by ADEKA Co., Ltd.).
Specific examples of the phosphorus-based antioxidant include IRGAFOS 168, IRGAFOS P-EPQ, IRGAFOS 126 (all of which are manufactured by BASF Co., Ltd.), Sumilizer BBM-S (manufactured by Sumitomo chemical Co., Ltd.), ADK STAB PEP-4C, ADK STAB PEP-8, ADK STAB PEP-36, ADK STAB HP-10, ADK STAB 1178, ADK STAB 2112, ADK STAB C, ADK STAB 135A, and ADK STAB 3010 (all of which are manufactured by ADEKA Co., Ltd.).
Specific examples of the sulfur-based antioxidant include IRGANOX PS800FL, IRGANOX PS802FL (BASF Co., Ltd.), Sumilizer WX (Sumitomo chemical Co., Ltd.), ADK STAB AO-503, and ADK STAB AO-23(ADEKA Co., Ltd.).
The lower limit of the total content of the antioxidant (C) is preferably 0.01 part by mass or more, and more preferably 0.2 part by mass, based on 100 parts by mass of the total of the base resins (a). This can reduce the occurrence of scorching when kneading the insulating resin composition, and can improve the thermal aging resistance of the insulating layer obtained by crosslinking the insulating resin composition. On the other hand, the upper limit of the total content of the antioxidant (C) is preferably 0.8 part by mass, and more preferably 0.6 part by mass, based on 100 parts by mass of the total of the base resins (a). This can reduce the amount of water generated during the crosslinking of the resin, and can also reduce bleeding from the crosslinked resin.
Further, the total content of the antioxidant (C) is more preferably 5 to 50 parts by mass with respect to 100 parts by mass of the crosslinking agent (B).
[ other component (D) ]
The insulating resin composition according to the present embodiment may contain other components as necessary. For example, various additives such as a moisture absorber, a heat stabilizer, a light stabilizer, a flame retardant, a softener, a filler, a colorant, a solvent, a pigment, a dye, and a phosphor can be added.
[ Properties of insulating resin composition ]
The insulating resin composition according to the present embodiment is preferably low in the electric field multiplying factor (maximum measured electric field/applied electric field) indicating the accumulation of space charge obtained by measuring the space charge by a pulse electrostatic stress method. In such a resin composition, when the insulating layer is formed, the amount of space charge accumulated in the insulating layer is reduced, and therefore, dielectric breakdown in the insulating layer can be made less likely to occur. Here, the electric field magnification of the insulating resin composition is preferably 130% or less. The resin composition having an electric field multiplying factor of less than 110% is particularly suitable as an insulating material for a DC power cable.
< method for producing insulating resin composition >
The method for producing the insulating resin composition according to the present embodiment includes two main methods. The method for producing the insulating resin composition of the 1 st embodiment is a method comprising: to a modified polyolefin resin modified with at least 1 selected from the group consisting of an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative, which are molecules having a polar group, an unmodified polyolefin resin, an antioxidant and, if necessary, a crosslinking agent are added, and then a base resin in which the modified polyolefin resin is diluted with the unmodified polyolefin resin is obtained. In this case, the method comprises a step of kneading the base resin so that the base resin has a so-called sea-island structure in which a second phase comprising the modified polyolefin resin is present in a first phase comprising the unmodified polyolefin resin and the average diameter of the second phase is 2 μm or less (production method (I)). The method for producing the second insulating resin composition is a method comprising: a method for producing a polyolefin resin pellet, which comprises adding an unmodified polyolefin resin and an antioxidant to a modified polyolefin resin modified with at least 1 selected from an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative, which are molecules having a polar group, to prepare a diluted polyolefin pellet comprising a base resin obtained by diluting the modified polyolefin resin with the unmodified polyolefin resin, and then adding a crosslinking agent to the prepared diluted polyolefin pellet as needed. In this case, the method comprises a step of dry-blending a base resin so that the base resin has a so-called sea-island structure in which a second phase containing a modified polyolefin resin is present in a first phase containing an unmodified polyolefin resin and the average diameter of the second phase is 2 μm or less (production method (II)).
{ Process (I) for producing insulating resin composition }
The method (I) for producing the insulating resin composition is a method comprising: an unmodified polyolefin resin, an antioxidant, and, if necessary, a crosslinking agent are added to a modified polyolefin resin modified with at least 1 selected from an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride, and an unsaturated dicarboxylic anhydride derivative, which are molecules having a polar group, and the mixture is kneaded, thereby obtaining a base resin in which the modified polyolefin resin is diluted with the unmodified polyolefin resin. The method comprises a step of kneading the base resin so that the base resin has a so-called sea-island structure in which a second phase comprising a modified polyolefin resin is present in a first phase comprising an unmodified polyolefin resin, and the second phase has an average diameter of 2 [ mu ] m or less.
(preparation and preparation of raw Material)
As the base resin (a), the crosslinking agent (B), and the antioxidant (C) used as raw materials in the method for producing an insulating resin composition according to the present embodiment, those described above can be used. Among them, as the modified polyolefin resin (a1) contained in the base resin (a), a modified polyolefin resin modified with at least 1 selected from the group consisting of an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride, and an unsaturated dicarboxylic anhydride derivative, which are molecules having a polar group, is used.
Here, the modification of the polyolefin resin based on the molecule having a polar group can be performed, for example, by: the above-mentioned unmodified polyolefin resin and the molecule having a polar group are melt-kneaded together with a small amount of a crosslinking agent for addition reaction by a single-screw or twin-screw extruder. In this case, in order to prevent abnormal crosslinking of the polyolefin resin, an antioxidant is preferably blended with the molecule having a polar group.
(kneading step)
In the kneading step of the method (I) for producing an insulating resin composition, an unmodified polyolefin resin (a2) and an antioxidant (C) are added to a modified polyolefin resin (a1) as a raw material of an insulating resin composition, and kneaded. In this case, the crosslinking agent (B) may be added and kneaded together with the unmodified polyolefin resin (A2) and the antioxidant (C). Thus, the modified polyolefin resin (a1) was diluted with the unmodified polyolefin resin (a2) to form the base resin (a), and the concentration of the polar group was adjusted to a desired range. At the same time, by kneading the modified polyolefin resin (a1) contained in the base resin (a) and the unmodified polyolefin resin (a2), a so-called sea-island structure in which a second phase (island phase) containing the modified polyolefin resin (a1) is present in a first phase (sea phase) containing the modified polyolefin resin (a2) can be formed, and the average diameter of the second phase (island phase) can be reduced.
Here, as for the kneading of the raw materials, the raw materials in which the crosslinking agent (B) is blended in advance as necessary with the base resin (a) and the antioxidant (C) may be kneaded. However, in particular, in the embodiment in which the crosslinking agent (B) is added, in order to suppress abnormal crosslinking of the base resin (a) due to thermal decomposition of the crosslinking agent (B) by heat at the time of kneading, it is preferable to knead raw materials including the base resin (a) and the antioxidant (C) first, and then add the crosslinking agent (B) to the kneaded mixture and knead the same.
The kneading of the raw materials of the insulating resin composition can be carried out by melt-kneading with a single-screw or twin-screw extruder. In particular, in order to prevent scorching of the resin due to the necessary or more shear heat, it is more preferable to perform melt kneading using a single-screw extruder.
As a screw used in a single-screw extruder, for example, as shown in fig. 5, it is preferable to use a screw 4 in which a resin mixing portion 43 of Madoc type, dullmadge type, or the like is provided at the middle portion or the tip portion of a full-flight screw 42. Here, if a screw 5 having a normal full-flight screw 52 as shown in fig. 6 is used, for example, the raw material containing at least the base resin (a) and the antioxidant (C) charged into the extruder is extruded forward at a constant speed only in the direction of the tip of the screw, and sufficient kneading cannot be expected. In contrast, in the present embodiment, by using the screw 4 provided with the resin mixing portion 43 of Madoc type, dullmadge type, or the like as shown in fig. 5, it is possible to cause a shearing force to strongly act on the raw material before the raw material charged into the extruder is extruded to the tip of the screw, and to increase the kneading time until the raw material is extruded, thereby making it possible to sufficiently knead the raw material.
In order to melt the polyolefin resin to obtain a viscosity capable of being stirred in a cylinder to an appropriate degree, the temperature of melt kneading at the time of modifying the polyolefin resin is preferably 140 ℃ or higher, and more preferably 160 ℃ or higher. On the other hand, in order to suppress the occurrence of scorch due to abnormal crosslinking, the upper limit of the temperature for melt kneading is preferably 300 ℃ or lower. In particular, from the viewpoint of rapidly completing a uniform reaction, the upper limit of the temperature for melt kneading is preferably 280 ℃ or lower.
As a method of mixing in the resin mixing section 54 of the screw 4, a position exchange method of promoting the position exchange of the raw material by complicating the flow place and thereby promoting the distribution mixing may be used, and for example, a screw of a dullmadge type, a DIS type, or a pin type may be used for the resin mixing section 43. Further, a barrier slit (barrier slit) system in which dispersion and mixing of the raw materials are promoted by strongly acting a shear stress may be used, and for example, a ring-type, Madoc-type, Unimelt-type or double-screw-type screw may be used for the resin mixing section 43. An elongation deformation method for promoting the dispersion and mixing of the raw materials by using an elongation flow may be used, and for example, a wave (wave) type, CTM type, pin (barrelpin) type, HM type, or Spirex type screw may be used for the resin mixing section 43.
The size of the portion of the screw 4 used for kneading is generally represented by the ratio of the length L to the diameter D (L/D ratio), and the L/D ratio is preferably 18 or more. In addition, the upper limit of the L/D ratio is preferably less than 40.
From the viewpoint of obtaining a uniform paste-like kneaded product, the kneading temperature in the kneading step is preferably higher than the melting point of at least one of the base resins (a). In particular, when kneading is performed while containing the crosslinking agent (B), the kneading temperature in the kneading step is preferably 130 ℃ or lower in order to avoid abnormal crosslinking of the base resin (a) due to thermal decomposition of the crosslinking agent (B). On the other hand, in the case where the crosslinking agent (B) is not contained, the kneading temperature in the kneading step may be higher than 130 ℃.
{ Process (II) for producing insulating resin composition }
The method (II) for producing the insulating resin composition is a method comprising: a method for producing a polyolefin resin pellet, which comprises adding an unmodified polyolefin resin and an antioxidant to a modified polyolefin resin modified with at least 1 selected from an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative, which are molecules having a polar group, to prepare a diluted polyolefin pellet comprising a base resin obtained by diluting the modified polyolefin resin with the unmodified polyolefin resin, and then adding a crosslinking agent to the prepared diluted polyolefin pellet. The method comprises a step of performing dry blending so that the base resin has a so-called sea-island structure in which a second phase comprising a modified polyolefin resin is present in a first phase comprising an unmodified polyolefin resin, and the average diameter of the second phase is 2 μm or less. That is, the method (II) for producing an insulating resin composition is different from the above-described method (I) for producing an insulating resin composition in that the method (I) for producing an insulating resin composition includes a step of adding an antioxidant (C) and a crosslinking agent (B) to a base resin (a) and kneading the mixture, and the method (II) for producing an insulating resin composition includes, instead of the step of kneading: an antioxidant (C) is added to the base resin (A) to prepare a diluted polyolefin pellet, and the prepared diluted polyolefin pellet is dry-blended with the crosslinking agent (B).
(Dry blending Process)
The dry blending step is as follows: the antioxidant (C) was added and the modified polyolefin resin (a1) diluted with the unmodified polyolefin resin (a2) was pelletized, and then, heating was performed in order to melt and absorb the crosslinking agent (B) into the pellets. In the dry blending step, in view of melting the crosslinking agent (B) and promoting absorption into the pellets, the heating is preferably performed to a temperature of not less than the melting point of the crosslinking agent (B), and more preferably to a temperature of not less than 10 ℃. On the other hand, in view of preventing abnormal crosslinking of the base resin (a), it is preferable that the heating temperature in dry blending is not higher than the decomposition temperature of the crosslinking agent (B).
For example, in the case of using dicumyl peroxide (DCP) as the crosslinking agent (B), the heating temperature at the time of dry blending is preferably heated to 40 ℃ or more, more preferably 50 ℃ or more, which is the melting point, in order to melt and rapidly absorb the DCP into the pellets. On the other hand, in order not to decompose DCP, it is preferable to dry-blend with the pellets at 130 ℃ or lower, which is the decomposition temperature of DCP.
Insulating tape for coating connection part of power cable
The insulating tape according to the present embodiment is made of the insulating resin composition described above, and can be used for coating a connection portion of a power cable. More specifically, it can be used for: an insulating layer covering the connection part is formed by laminating an inner semiconductive layer as necessary on the outer periphery of the connection part in which the exposed end parts of the conductors of the plurality of power cables are connected to each other by the conductors.
In order to reduce the number of windings when wound around the connection portion, the tape thickness of the insulating tape according to the present embodiment is preferably 30 μm or more, more preferably 50 μm or more, and still more preferably 70 μm or more. On the other hand, in order to facilitate winding around the connection portion, the upper limit of the tape thickness of the insulating tape is preferably 250 μm or less, more preferably 200 μm or less, and further preferably 150 μm or less.
In addition, the tape width of the insulating tape according to the present embodiment is preferably 3mm or more and 40mm or less in order to form a smooth winding surface.
The insulating tape according to the present embodiment is suitably used for an application in which an insulating layer is formed by winding around the outer periphery of a connection portion in which exposed end portions of conductors of a plurality of power cables are connected to each other by conductors. In particular, if the stretching of the tape when the tape is wound and the melt flow of the resin when the base resin (a) is crosslinked do not occur, the outer periphery of the connecting portion may be covered with the insulating layer in a state having a desired sea-island structure.
< method for producing insulating tape >
The method for producing the insulating tape according to the present embodiment is not particularly limited, and includes, for example, the following steps: a step of forming a film by extrusion molding the insulating resin composition, and cooling the surface temperature of the film to the melting point of the unmodified polyolefin resin or less within 15 seconds after the insulating resin composition is extruded; and a step of slitting the cooled film to form a tape.
As means for extrusion molding for forming a film of a predetermined thickness from the insulating resin composition, an inflation method, a T-die method, a casting method, a calendering method, and the like can be used, and among them, an inflation method is preferably used.
When the polyethylene resin is contained as the base resin (a) in the film formation, the temperature of the die for extrusion molding of the insulating resin composition is preferably 120 ℃. This enables formation of a band having a sea-island structure including a second phase (island phase) having a small average diameter. On the other hand, the upper limit of the temperature of the mold when the crosslinking agent (B) is added is preferably 150 ℃ or less, and more preferably 140 ℃ or less, in order to reduce decomposition of the crosslinking agent (B) contained in the insulating resin composition.
The surface temperature of the film formed is cooled to the melting point of the unmodified polyolefin resin (a2) or less within 15 seconds, more preferably within 10 seconds after the insulating resin composition is extruded. This can suppress the growth of the second phase (island phase) contained in the insulating tape to be formed, and therefore, even when the connecting portion of the power cable is wound with the insulating tape, the insulating tape can have a desired sea-island structure, and an insulating layer in which insulation breakdown is less likely to occur can be obtained.
Examples of the method of cooling the film include a method of adjusting the temperature and distance of a roller with which the film first contacts, a method of air-cooling the surface of the film, a method of lowering the temperature of a working environment, and a method of pressing a radiation cooling plate against the film. Among these, particularly in the case of forming a film by the inflation method, a method of reducing the temperature of air used when the film is inflated is preferable in terms of enabling accurate temperature adjustment.
Further, the film formed of the insulating resin composition is slit so as to have a predetermined tape width before and after cooling the film, and is molded into a tape.
< Power Cable (first embodiment) >
As shown in fig. 2(a) and 2(b), the power cable 2 according to the present embodiment includes: a conductor 21; and a composite coating film 20, wherein the composite coating film 20 is formed by sequentially laminating an inner semiconductive layer 22 formed of a first conductive resin, an insulating layer 23, and an outer semiconductive layer 24 formed of a second conductive resin on the outer periphery of a conductor 21, and the insulating layer 23 is formed by using the insulating resin composition as a raw material and crosslinking at least a modified polyolefin resin (a2) in the second phase (island phase) and at least an unmodified polyolefin resin (a1) in the first phase (sea phase).
As shown in fig. 2(b), in the power cable 2, an inner semiconductive layer 22, an insulating layer 23, and an outer semiconductive layer 24 are sequentially laminated on the outer periphery of a conductor 21, and the inner semiconductive layer 22, the insulating layer 23, and the outer semiconductive layer 24 constitute a composite coating 20. Preferably, a metal shield layer 25 and a sheath 26 are laminated in this order on the composite coating 20.
(insulating layer)
Among them, the insulating layer 23 is preferably formed by winding and crosslinking an insulating tape for forming an insulating layer having a tape thickness in the range of 30 μm to 250 μm and a tape width in the range of 3mm to 40mm around the outer periphery of the inner semiconductive layer 22. The insulating layer 23 is formed from a layer obtained by using the insulating resin composition as a raw material and crosslinking at least the modified polyolefin resin (a2) in the second phase (island phase) in the sea-island structure and at least the unmodified polyolefin resin (a1) in the first phase (sea phase) respectively.
From the viewpoint of insulating properties, the thickness of the insulating layer 23 is preferably 1.5mm or more, more preferably 5mm or more, and further preferably 15mm or more. On the other hand, from the viewpoint of laying workability, the upper limit of the thickness of the insulating layer 23 is preferably 100mm or less, and more preferably 50mm or less.
(inner and outer semi-conducting layers)
The inner semiconductive layer 22 and the outer semiconductive layer 24 are each composed of a first conductive resin and a second conductive resin, each of which is made of, for example, a semiconductive resin composition containing a crosslinkable resin, conductive carbon black, and, if necessary, a crosslinking agent, and at least the crosslinkable resin is crosslinked. Here, examples of the crosslinkable resin include at least one resin selected from the group consisting of an ethylene-vinyl acetate copolymer, an ethylene-methyl acrylate copolymer, an ethylene-ethyl acrylate copolymer, and an ethylene-butyl acrylate copolymer.
The thicknesses of the inner semiconductive layer 22 and the outer semiconductive layer 24 are each preferably 0.1mm or more, and more preferably 0.5mm or more, from the viewpoint of suppressing the variation in electric field by utilizing their conductive properties. From the viewpoint of quickly releasing heat generated when a power cable is energized, the upper limits of the thicknesses of the inner semiconductive layer 22 and the outer semiconductive layer 24 are each preferably 3mm or less, more preferably 2mm or less, and still more preferably 1mm or less.
The total thickness of the inner semiconductive layer 22 and the outer semiconductive layer 24 is preferably 5mm or less, more preferably 4mm or less, and still more preferably 3mm or less. Thus, even when the semiconductive resin composition as a material of the inner semiconductive layer 22, the insulating resin composition as a material of the insulating layer 23, and the semiconductive resin composition as a material of the outer semiconductive layer 24 are laminated on the conductor 21 and then the insulating resin composition is crosslinked, the insulating resin composition is easily cooled, and therefore, the growth of the second phase (island phase) of the sea-island structure can be suppressed. On the other hand, if the total thickness is large, the cooling of the insulating resin composition is slow, and thus the second phase (island phase) of the sea-island structure tends to grow.
(Metal Shield layer and resist sheath)
A metal shield layer and a resist sheath (both not shown) may be provided around the outer semiconductive layer 24. As the metal shield layer, a layer formed of, for example, lead, copper, or aluminum can be used. As the resist sheath, for example, a sheath made of vinyl chloride, polyethylene, or nylon can be used.
< method for manufacturing power cable >
The method for manufacturing a power cable according to the present embodiment is, for example, a method for manufacturing a power cable 2 shown in fig. 2(a) and 2(b), and includes the steps of: an inner semiconductive layer 22, an insulating layer 23, and an outer semiconductive layer 24 are sequentially laminated on the outer periphery of the conductor 21, and at least the insulating layer 23 is crosslinked.
(lamination of inner semiconductive layer, insulating layer and outer semiconductive layer)
The inner semiconductive layer 22 can be laminated by, for example, extrusion molding in which a semiconductive resin composition containing a crosslinkable resin, conductive carbon black, and, if necessary, a crosslinking agent is extruded to the outer periphery of the conductor 21. The insulating layer 23 can be laminated by extrusion molding the insulating resin composition on the outer periphery of the semiconductive resin composition that is a material of the inner semiconductive layer 22. The outer semiconductive layer 24 can be laminated by extrusion molding of a semiconductive resin composition similar to the inner semiconductive layer 22 on the outer periphery of an insulating resin composition that is a material of the insulating layer 23. The inner semiconductive layer 22, the insulating layer 23, and the outer semiconductive layer 24 may be formed by extrusion molding on the outer circumference of the conductor 21 at the same time.
The temperature of the resin in the extrusion molding is preferably 110 ℃ or higher, and more preferably 120 ℃ or higher, when the polyethylene resin is contained as the base resin (a). In addition, the temperature of the resin at the time of extrusion molding is preferably 140 ℃ or lower, more preferably 130 ℃ or lower, from the viewpoint of suppressing the crosslinking reaction of the base resin (a).
Here, the laminated insulating layer 23 is cooled to the melting point of the unmodified polyolefin resin (a2) or less within 15 seconds, more preferably within 10 seconds, after being extruded to the outer periphery of the conductor 21 and the inner semiconductive layer 22. This can suppress the growth of the second phase (island phase) in the sea-island structure formed in the insulating resin composition, and thus can provide the insulating layer 23 in which dielectric breakdown is less likely to occur. The insulating layer 23 may be cooled by air-cooling the surface of the resin, reducing the temperature of the working environment, pressing a radiation cooling plate, or the like.
(crosslinking of insulating layer)
Next, when the semiconductive resin composition contains a crosslinking agent (B), the following crosslinking step is performed: the laminated insulating layer 23 is subjected to pressure-heat treatment under conditions of 300kPa or more and 5000kPa or less and 140 ℃ or more and 280 ℃ or less to crosslink the modified polyolefin resin (a1) and the unmodified polyolefin resin (a2) contained in the insulating layer 23. This can improve the mechanical properties and heat resistance of the insulating layer 23.
In the crosslinking step, the pressure vessel is sealed and filled with a gas, and the pressure and heat treatment is performed in a pressurized state. In this case, the pressure at the time of the pressure-heat treatment in the crosslinking step is preferably 300kPa or more, and more preferably 400kPa or more. In addition, the pressure at the time of the pressure heating treatment is preferably 5000kPa or less, more preferably 1000kPa or less, from the viewpoint of preventing the seal of the closed portion of the pressure vessel from being broken in the crosslinking step.
In order to promote the crosslinking reaction by the action of the crosslinking agent, the heating temperature in the crosslinking step is preferably 140 ℃ or higher, and more preferably 160 ℃ or higher. On the other hand, the heating temperature in the crosslinking step is preferably 280 ℃ or less, more preferably 260 ℃ or less, from the viewpoint of preventing thermal decomposition of the polyolefin resin.
< Power Cable (second embodiment) >
As shown in fig. 3(a), the power cable 3 according to the present embodiment includes a connection structure portion 37. The connection structure portion 37 includes: a connection section (joint section) 371 in which the ends of the conductors of the plurality of power cables (here, 2 conductors 31a and 32a in fig. 3) exposed are conductor-connected to each other; and a composite coating 370, wherein the composite coating 370 is formed by sequentially laminating an inner semiconductive layer 372 formed of a first conductive resin, an insulating layer 373, and an outer semiconductive layer 374 formed of a second conductive resin on the outer periphery of the connecting portion 371, and the insulating layer 373 is formed by using the insulating resin composition as a raw material and crosslinking at least a modified polyolefin resin (a1) in the second phase (island phase) and at least an unmodified polyolefin resin (a2) in the first phase (sea phase).
In the power cable 3, as shown in fig. 3(a) and 3(c), an inner semiconductive layer 372, an insulating layer 373, and an outer semiconductive layer 374 are sequentially stacked on the outer periphery of the connection portion 371, and these layers constitute a connection structure portion 17.
(insulating layer)
From the viewpoint of insulating properties, the thickness of the insulating layer 373 covering the outer periphery of the connection portion 371 is preferably 1.5mm or more, more preferably 5mm or more, and further preferably 15mm or more. From the viewpoint of laying workability, the upper limit of the thickness of the insulating layer 373 is preferably 100mm or less, and more preferably 50mm or less.
The insulating layer 373 may be formed by winding the insulating tape for forming an insulating layer around the outer circumference of the inner semiconductive layer 372 and crosslinking the wound insulating tape. In this embodiment, since the insulating layer 373 having a desired sea-island structure can be formed from the insulating tape for insulating layer formation, the insulating layer 373 can be formed by a simple method, and dielectric breakdown in the formed insulating layer 373 can be reduced. Here, as described above, the insulating tape for forming the insulating layer 373 preferably has a tape thickness in the range of 30 μm to 250 μm, and a tape width in the range of 3mm to 40 mm.
(inner and outer semi-conducting layers)
The inner semiconductive layer 372 and the outer semiconductive layer 374 covering the outer periphery of the connection portion 371 may be the same layers as those of the inner semiconductive layer and the outer semiconductive layer in the first embodiment. Here, the thicknesses of the inner semiconductive layer 372 and the outer semiconductive layer 374 are each preferably 0.1mm or more, and more preferably 0.5mm or more, from the viewpoint of suppressing the electric field unevenness by utilizing their conductive properties. From the viewpoint of quickly releasing heat generated when a power cable is energized, the upper limits of the thicknesses of the inner semiconductive layer 372 and the outer semiconductive layer 374 are each preferably 3mm or less, more preferably 2mm or less, and even more preferably 1mm or less.
In addition, the total thickness of the inner semiconductive layer 372 and the outer semiconductive layer 374 is preferably 5mm or less, more preferably 4mm or less, and further preferably 3mm or less, as in the inner semiconductive layer and the outer semiconductive layer of the first embodiment.
(Metal Shield layer and resist sheath)
As in the power cable of the first embodiment, a metal shield layer and a resist sheath (both not shown) may be provided around the outer semiconductive layer 374.
Method for forming insulating layer on outer surface of connection part of power cable
The method for forming an insulating layer on an outer surface of a connection portion of a power cable according to the present embodiment includes the steps of: a tape winding step of winding the insulating tape around an outer periphery of a connection portion in which exposed end portions of conductors of a plurality of power cables are connected to each other by conductors, thereby forming an insulating layer on an outer surface of the connection portion; and a crosslinking step of subjecting the connecting portion on which the insulating layer is formed to a pressure-heating treatment under conditions of 300kPa to 5000kPa inclusive and 140 ℃ to 280 ℃ inclusive to crosslink the unmodified polyolefin resin and the modified polyolefin resin contained in the insulating layer.
Fig. 4 is a diagram illustrating an insulating layer forming method according to the present invention. In fig. 4, the following is shown as an example: a power cable 30a in which an inner semiconductive layer 32a, an insulating layer 33a, an outer semiconductive layer 34a, a metal shield layer 35a, and a sheath 36a are sequentially laminated around a conductor 31a made of copper, aluminum, or the like, and a power cable 30b in which an inner semiconductive layer 32b, an insulating layer 33b, an outer semiconductive layer 34b, a metal shield layer 35b, and a sheath 36b are sequentially laminated around a conductor 31b are connected.
(formation of connecting part)
As shown in fig. 4(a), the plurality of power cables 30a and 30b to be connected have end conductors 31a and 31b exposed, respectively. At this time, the lengths of the exposed portions are denoted by E1 and E2, respectively. Here, when the insulating layers 33a and 33b are formed of a resin having high hydrophilicity, particularly the modified polyethylene resin (a1), it is preferable that the insulating layers 33a and 33b are also exposed together with the conductors 31a and 31 b. Since the insulating tape is wound and laminated around the exposed insulating layers 33a and 33b, the adhesion between the insulating layers 33a and 33b and the insulating tape can be improved, and thus dielectric breakdown at the interface therebetween can be made less likely to occur.
Next, as shown in fig. 4(b), the ends of the conductors 31a and 31b are conductor-connected (joined). As a method of conductor connection, for example, welding may be used, and the connection portion (welded portion) 371 may be formed by conductor connection.
(formation of inner semiconductive layer)
On the outer periphery of the formed connection portion 371, an inner semiconductive layer 372 can be formed as shown in fig. 4 (c). The inner semiconductive layer 372 is formed of a semiconductive resin composition containing, for example, a crosslinkable resin and conductive carbon black, and, if necessary, a crosslinking agent.
The inner semiconductive layer 372 can be obtained by, for example, molding a resin, and more specifically, can be formed by extruding a resin on the surfaces of the conductors 31a and 31b, or can be formed by inserting the conductors 31a and 31b into a mold and injecting the resin into the mold, or can be formed by winding a resin in a band shape around the surfaces of the conductors 31a and 31 b. Further, a semiconductive pipe that shrinks by heating may be inserted in advance into either of the conductors 31a and 31b before the connection portion 371 is formed, and the inner semiconductive layer 372 may be formed by heating and shrinking the pipe after the connection portion 371 is formed.
(formation of insulating layer)
Next, as shown in fig. 4(d), an insulating layer 373 is formed on the outer periphery of the inner semiconductive layer 372 formed on the outer periphery of the connection portion 371 (which is formed by conductor-connecting the exposed end portions of the conductors 31a and 31b of the plurality of power cables 30a and 30 b) over a range covering the entire outer peripheries of the connection portion 371 and the inner semiconductive layer 372.
As a method for forming the insulating layer 373, it is preferable to wind an insulating tape, which is made of the insulating resin composition described above, having a tape thickness of 30 μm or more and 250 μm or less and a tape width of 3mm or more and 40mm or less around the surfaces of the conductors 31a and 31b so that the insulating layer 373 can be formed by a simple method. On the other hand, the insulating layer 373 may be formed by extrusion molding an insulating resin composition on the surfaces of the conductors 31a and 31b and the inner semiconductive layer 372, similarly to the insulating layer of the power cable (for example, the insulating layer 23 in fig. 2 (a)). The insulating layer 373 can be formed by inserting the conductors 31a and 31b having the inner semiconductive layer 372 into a mold and injecting an insulating resin composition into the mold.
(formation of outer semiconductive layer)
Next, an outer semiconductive layer 374 is formed around the insulating layer 373 as shown in fig. 4 (e). The outer semiconductive layer 374 is formed of a semiconductive resin composition in the same manner as the inner semiconductive layer 372.
The outer semiconductive layer 374 can be obtained by, for example, molding a resin, like the inner semiconductive layer 372. In addition, a semiconductive pipe that shrinks by heating may be inserted into the conductors 31a and 31b before the connection portion 371 is formed, and the pipe may be shrunk by heating after the connection portion 371 is formed.
(crosslinking step)
Next, in the case where the resin composition constituting the insulating layer 373 contains the crosslinking agent (B), the following crosslinking step is performed: the connection portion 371 on which the insulating layer 373 is formed is subjected to pressure-heat treatment under conditions of 300kPa or more and 5000kPa or less and 140 ℃ or more and 280 ℃ or less, thereby crosslinking the polyethylene contained in the insulating layer 373. Thus, the modified polyethylene resin (a1) and the unmodified polyethylene resin (a2) are crosslinked, whereby the mechanical properties and heat resistance of the resin material constituting the insulating layer 373 can be improved.
In the crosslinking step, the pressure vessel is sealed and filled with a gas, and the pressure and heat treatment is performed in a pressurized state. In this case, the pressure at the time of the pressure-heat treatment in the crosslinking step is preferably 300kPa or more, and more preferably 400kPa or more. In addition, the pressure at the time of the pressure heating treatment is preferably 5000kPa or less, more preferably 1000kPa or less, from the viewpoint of preventing the seal of the closed portion of the pressure vessel from being broken in the crosslinking step.
In order to promote the crosslinking reaction by the action of the crosslinking agent, the heating temperature in the crosslinking step is preferably 140 ℃ or higher, and more preferably 160 ℃ or higher. On the other hand, the heating temperature in the crosslinking step is preferably 280 ℃ or less, more preferably 260 ℃ or less, from the viewpoint of preventing thermal decomposition of the polyethylene resin.
(formation of Metal Shield layer and resist sheath)
A metal shield layer and a resist sheath (both not shown) may be provided around the crosslinked insulating layer 373. As the metal shield layer, a layer formed of, for example, lead, copper, or aluminum can be used. As the resist sheath, for example, a sheath made of vinyl chloride, polyethylene, or nylon can be used.
Examples
Next, examples of the present invention and comparative examples will be described in order to make the effects of the present invention more clear, but the present invention is not limited to these examples.
[ inventive example 1]
(preparation of insulating resin composition)
As the base resin (A), 5 parts by mass of a maleic anhydride-modified Polyethylene "SCONA TSPE 1112 GALL" (manufactured by BYK Chemie Japan K.K., melting point 115 to 132 ℃ C., specific gravity 0.89 to 0.94) as the modified polyolefin resin (A1) and 95 parts by mass of a low-density Polyethylene "ZF 30R" (manufactured by Japan Polyethylene Corporation, melting point 110 ℃ C., specific gravity 0.92) as the unmodified polyolefin resin (A2) were used, and the total content thereof was 100 parts by mass.
To 100 parts by mass of the base resin (a), 0.2 part by mass of "IRGAFOS P-EPQ" (tetrakis (2, 4-di-tert-butylphenyl) -biphenylene diphosphonite, manufactured by BASF corporation) as a phosphorus antioxidant was added as an antioxidant (C), and melt-kneaded and pelletized using a single screw extruder provided with a screw (IKG corporation, L/D ratio 25) having a Madoc-type resin mixing section in the middle of a full-flight screw at an extrusion temperature (kneading temperature) of 125 ℃.
To the obtained pellets was dry-blended 1.7 parts by mass of "Percumyl D" (dicumyl peroxide (DCP), manufactured by japan oil and fat co., melting point 40 ℃, decomposition temperature 130 ℃) as a crosslinking agent (B) at 90 ℃ to allow the molten DCP to be absorbed into the pellets, thereby obtaining an insulating resin composition (melting point 110 ℃).
(formation of sheet for evaluation)
The obtained insulating resin composition was extrusion-molded by a T-die method so that the temperature of the die was 130 ℃ and the film thickness was 0.3 mm. At this time, the film was cooled while adjusting the temperature and distance of the roller with which the film first contacted so that the surface temperature of the film became the melting point of the unmodified polyolefin resin (a2) or less 10 seconds after the insulating resin composition was extruded.
The obtained film was subjected to a pressure-heat treatment by pressurizing at 170 ℃ and under a pressure of 5000kPa for 30 minutes to crosslink the modified polyolefin resin (A1) and the unmodified polyolefin resin (A2), thereby obtaining a 0.3mm thick sheet for evaluation comprising a resin crosslinked body.
The obtained evaluation sheet was cut into thin pieces, and RuO was used4After the metal staining, the sea-island structure of the resin was photographed using a transmission electron microscope (TEM, HT7700 manufactured by Hitachi High-Technologies Corporation). The sea-island structure was photographed as follows: the contrast was adjusted so that the sea-island structure could be identified from the cross section of the resin by setting the magnification of the microscope to 10000 times. The captured image was analyzed by using image analysis software ImageJ, and the average diameter of the island phases included in the image was determined. Here, the diameter of the island phase is determined by image processing by ImageJ, and the arithmetic average of the maximum size and the minimum size is determined by using the maximum size and the minimum size as the maximum size and the minimum size, respectively, when the size of the island phase is measured over the entire circumference (360 degrees). In addition, the number of island phases having a diameter of 0.5 to 2.0 μm is determined for an arbitrary observation range of 10 μm in vertical direction × 10 μm in horizontal direction included in the captured image, and the sum of the areas occupied by all the island phases is determined. When the inter-particle distances are separated by not less than 1/50, which is the average particle diameter, the analysis is performed as islands independent from each other.
The average diameter of the island phases in the sea-island structure of the evaluation sheet obtained as described aboveThe diameter is 1 μm. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in an observation range of 10 μm in vertical direction × 10 μm in horizontal direction is 6, and the sum of the areas of all the island phases is 5 μm2。
[ inventive example 2]
To 100 parts by mass of the base resin (a), as the antioxidant (C), "IRGANOX 1010" (pentaerythritol tetrakis [3- (3 ', 5 ' -di-tert-butyl-4 ' -hydroxyphenyl) propionate) as a phenolic antioxidant was used and added]Ciba specialty chemicals inc.) was used in the same manner as in invention example 1 except that the amount of the resin composition was 0.2 parts by mass, to obtain a sheet for evaluation comprising a resin crosslinked body. The average diameter of the island phases in the sea-island structure of the obtained evaluation sheet, which was determined by the same method as in inventive example 1, was 1 μm. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in an observation range of 10 μm in vertical direction × 10 μm in horizontal direction is 5, and the sum of the areas of all the island phases is 5 μm2。
[ inventive example 3]
An insulating resin composition was prepared in the same manner as in invention example 1, except that 5 parts by mass of an ethylene-methacrylic acid copolymer "HIMILAN 1705 Zn" (Dupont-Mitsui polymeric co., ltd., methacrylic acid content 15 mass%, melting point 91 ℃, specific gravity 0.95) as the modified Polyethylene (a1) and 95 parts by mass of a low-density Polyethylene "ZF 30R" (manufactured by Japan Polyethylene Corporation, melting point 110 ℃, specific gravity 0.92) as the unmodified Polyethylene (a2) were used as the base resin (a), and the total was 100 parts by mass.
An evaluation sheet formed of a resin crosslinked body was obtained in the same manner as in invention example 1, except that the film was cooled so that the surface temperature of the film became the melting point of the unmodified polyolefin resin (a2) or less 3 seconds after the insulating resin composition was extruded. The average diameter of the island phases in the sea-island structure of the obtained evaluation sheet, which was determined by the same method as in inventive example 1, was 2 μm. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in the observation range of 10 μm in vertical direction × 10 μm in horizontal direction is 5, and all the island phases are arrangedThe sum of the occupied areas is 6 mu m2。
[ inventive example 4]
As the base resin (A), 30 parts by mass of a maleic anhydride-modified polypropylene "Youmex 100 TS" (melting point 136 ℃ C., specific gravity 0.89, manufactured by Sanyo chemical Co., Ltd.) as the modified polyolefin resin (A1) and 70 parts by mass of a polypropylene (melting point 167 ℃ C., specific gravity 0.925, Melt Index (MI)0.8) as the unmodified polyolefin resin (A2) were used, and the total content thereof was 100 parts by mass.
To 100 parts by mass of the base resin (a), 0.2 part by mass of "IRGAFOSP-EPQ" (tetrakis (2, 4-di-tert-butylphenyl) -biphenylene diphosphonite, manufactured by BASF corporation) as a phosphorus antioxidant was added as an antioxidant (C), and melt-kneaded and pelletized using a single screw extruder provided with a screw (IKG corporation, L/D ratio 28) having a Madoc-type resin mixing section in the middle of a full-flight screw at an extrusion temperature (kneading temperature) of 220 ℃. The obtained insulating resin composition was extrusion-molded by a T-die method in the same manner as in inventive example 1, and the obtained film was used as a sheet for evaluation.
The average diameter of the island phases in the sea-island structure of the obtained evaluation sheet, which was determined by the same method as in inventive example 1, was 2 μm. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in an observation range of 10 μm in vertical direction × 10 μm in horizontal direction is 20, and the sum of the areas of all the island phases is 20 μm2。
Comparative example 1
In the same manner as in invention example 1 except for the following points, a sheet for evaluation formed of a resin crosslinked body was obtained: a low-density Polyethylene "ZF 30R" (manufactured by Japan Polyethylene Corporation, melting point 110 ℃, specific gravity 0.92) as an unmodified Polyethylene (a2) was used as the base resin (a) without using the modified Polyethylene (a1), and the content thereof was 100 parts by mass; and a full-flight screw (manufactured by IKG corporation, L/D ratio 25) having no resin mixing portion was used as a screw for melt-kneading the raw material. In the obtained evaluation sheet, no sea-island structure was formed.
Comparative example 2
As a screw for melt-kneading the raw material, a full-flight screw (manufactured by IKG corporation, L/D ratio: 16) having no resin mixing portion was used, and except for the above, a sheet for evaluation formed of a resin crosslinked body was obtained in the same manner as in example 1 of the present invention. The average diameter of the island phases in the sea-island structure of the obtained evaluation sheet, which was determined by the same method as in inventive example 1, was 13 μm. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in an observation range of 10 μm in the vertical direction × 10 μm in the horizontal direction is 0, and the sum of the areas of all the island phases is 25 μm2。
Comparative example 3
In the same manner as in invention example 1 except for the following points, a sheet for evaluation formed of a resin crosslinked body was obtained: a fully-threaded screw (manufactured by IKG corporation, L/D ratio 25) having no resin mixing portion was used as a screw for melt-kneading the raw material; and, in the case of extrusion molding of the insulating resin composition, the film is cooled by adjusting the temperature and distance of the roller with which the film first comes into contact so that the surface temperature of the film becomes equal to or lower than the melting point of the unmodified polyolefin resin (a2) 18 seconds after the insulating resin composition is extruded. The average diameter of the island phases in the sea-island structure of the obtained evaluation sheet, which was determined by the same method as in inventive example 1, was 3 μm. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in the observation range of 10 μm in the vertical direction × 10 μm in the horizontal direction is 4, and the sum of the areas of all the island phases is 4 μm2。
[ inventive example 5]
The insulating resin composition obtained in example 1 of the present invention was used as an insulating resin composition for forming an insulating layer, and a resin composition containing a crosslinkable resin, conductive carbon black and a crosslinking agent was used as a semiconductive resin composition for forming an inner semiconductive layer and an outer semiconductive layer.
The cross-sectional area of the conductor is 2000mm2The semiconductive resin composition forming the inner semiconductive layer, the insulating resin composition of invention example 1 forming the insulating layer, and the semiconductive resin composition forming the outer semiconductive layer were extrusion-molded in 3 layers simultaneously on the outer peripheral surface of a conductor having a length of 25 m. At this time, the resin thickness of the inner semiconductive layer was set to 1.5mm, the resin thickness of the insulating layer was set to 15mm, the resin thickness of the outer semiconductive layer was set to 1.5mm, and the temperature of the mold was set to 128 ℃. Further, after 10 seconds after the extrusion of these resins, the surface temperature of the extruded resin was cooled to the melting point of the unmodified polyolefin resin (a2) or less.
Next, the insulating resin composition of invention example 1, which forms the insulating layer, was crosslinked by performing a heating treatment under a nitrogen atmosphere at a pressure of 784kPa and a heating temperature of 220 ℃ for 2 hours, and the inner semiconductive layer, the insulating layer, and the outer semiconductive layer were formed on the outer peripheral surface of the conductor.
A metal shield layer and a resist sheath were provided around the outer semiconductive layer thus formed, thereby obtaining a power cable 2 having a structure shown in fig. 2(a) and (b). The average diameter of the island phases in the sea-island structure, which was determined by the same method as in inventive example 1 using the insulating layer 23 of the obtained power cable as an evaluation sheet, was 1 μm. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in the observation range of 10 μm in the vertical direction × 10 μm in the horizontal direction is 10, and the sum of the areas of all the island phases is 11 μm2。
[ inventive example 6]
A power cable was obtained in the same manner as in invention example 5 except that, when the semiconductive resin composition forming the inner semiconductive layer, the insulating resin composition forming the insulating layer obtained in invention example 1, and the semiconductive resin composition forming the outer semiconductive layer were simultaneously extrusion-molded in 3 layers, the resin thickness of the inner semiconductive layer was 2mm and the resin thickness of the outer semiconductive layer was 2.5 mm. The average diameter of the island phases in the sea-island structure, which was determined by the same method as in inventive example 1 using the insulating layer of the obtained power cable as an evaluation sheet, was 2 μm. The number of island phases having a diameter of 0.5 to 2.0 μm in the observation range of 10 μm in the vertical direction × 10 μm in the horizontal direction was 7, and the sum of the areas of all the island phases was 8 μm2。
[ inventive example 7]
An insulating tape was produced using the resin composition obtained in inventive example 1. Here, in the extrusion molding of the insulating resin composition, a film was formed using an inflation film-making machine (manufactured by PLACO corporation) under such conditions that the temperature of the die at the time of extrusion molding was 130 ℃, the film thickness was 100 μm, and the surface temperature of the film after 10 seconds from the extrusion became the melting point of the unmodified polyolefin resin (a2) or less. The obtained film was slit so that the tape width became 20mm, thereby obtaining an insulating tape having the same thickness as the film (i.e., 100 μm). The average diameter of the island phases in the sea-island structure of the obtained insulating tape as an evaluation sheet was 1 μm, which was determined by the same method as in inventive example 1. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in an observation range of 10 μm in vertical direction × 10 μm in horizontal direction is 6, and the sum of the areas of all the island phases is 6 μm2。
Comparative example 4
An insulating tape was obtained in the same manner as in invention example 7, except for the following points: the same insulating resin composition as that used in inventive example 2; a fully-threaded screw (manufactured by IKG corporation, L/D ratio 24) having no resin mixing portion was used as a screw for melt-kneading the raw material; and, in the case of extrusion molding of the insulating resin composition, the film is formed under such a condition that the surface temperature of the film 16 seconds after the extrusion is not more than the melting point of the unmodified polyolefin resin (a 2). The average diameter of the island phases in the sea-island structure of the obtained insulating tape as an evaluation sheet was 5 μm, which was determined by the same method as in inventive example 1. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in the observation range of 10 μm in the vertical direction × 10 μm in the horizontal direction is 2, and the sum of the areas of all the island phases is 15 μm2。
[ inventive example 8]
Using 2 the power cable manufactured in invention example 5, as shown in fig. 4(a), the conductors 31a, 31b at the respective ends were exposed by cutting, and then one of the power cables was inserted into a shrinkable tube having a thickness of 1mm to be an outer semiconductive layer. Next, as shown in fig. 4(b), the ends of the conductors 31a and 31b are conductor-connected to form a connection portion 371, and then, as shown in fig. 4(c), a semiconductive tape is wound so as to cover the exposed portions of the conductors 31a and 31b, thereby forming an inner semiconductive layer 372 having a thickness of 1 mm. Then, the insulating tape of example 7 of the present invention was wound so as to further cover the outer periphery of the formed inner semiconductive layer 372, and an insulating layer 373 having a thickness of 20mm was laminated and covered with the above-described shrink tube to form an outer semiconductive layer 374.
Next, by performing heating treatment of 784kPa pressure and 220 ℃ heating temperature for 3 hours in a nitrogen atmosphere, the insulating resin composition contained in the insulating tape was crosslinked, and thereby an inner semiconductive layer, an insulating layer, and an outer semiconductive layer were formed on the outer peripheral surface of the conductor.
A metal shield layer and a resist sheath were provided around the outer semiconductive layer thus formed, whereby 1 power cable having the structure shown in fig. 3(a) to (c) and connected thereto was obtained. The average diameter of the island phase in the sea-island structure obtained by using the insulating layer 372 of the covered connection portion 371 of the obtained power cable as an evaluation sheet by the same method as that of example 1 of the present invention was 1 μm. The number of island phases having a diameter of 0.5 to 2.0 μm in the observation range of 10 μm in the vertical direction × 10 μm in the horizontal direction was 8, and the sum of the areas of all the island phases was 7 μm2。
Comparative example 5
An insulating tape was produced in the same manner as in invention example 7 except for the following points, and 2 power cables were connected to 1 cable using the insulating tape in the same manner as in invention example 8: a fully-threaded screw (manufactured by IKG corporation, L/D ratio 24) having no resin mixing portion was used as a screw for melt-kneading the raw material; and, in extrusion molding of the insulating resin composition, the surface temperature of the film 16 seconds after extrusion is not more than the melting point of the unmodified polyolefin resin (A2)The condition of (1) forms an aspect of a film. The average diameter of the island phase in the sea-island structure, which was determined by the same method as in example 1 of the present invention, was 6 μm using the insulating layer of the coated connection portion of the obtained power cable as an evaluation sheet. In addition, the number of island phases having a diameter of 0.5 to 2.0 μm in the observation range of 10 μm in the vertical direction × 10 μm in the horizontal direction is 1, and the sum of the areas of all the island phases is 21 μm2。
[ evaluation of electric field multiplying factor ]
The field increase rates of the evaluation sheets, the insulating tapes, and the insulating layers of the power cables (the insulating layers of the covered connection portions of the power cables in the present invention examples 8 and the comparative examples 5) according to the present invention examples and the comparative examples were evaluated by a pulse electrostatic stress method.
A sample of the sheet for evaluation, the insulating tape and the insulating layer to be measured was cut into pieces having an aspect ratio of 50mm and a thickness of 0.3mm, and sandwiched between an upper electrode and a lower electrode of a space charge measuring apparatus (Five Lab Co., Ltd., Standard PEA-ST), and a negative 30kV/mm direct current electric field was continuously applied to the crosslinked material sheet at a temperature of 90 ℃ for 48 hours, and the ratio of the measured maximum measured electric field to the applied electric field was defined as "electric field gain ratio". Here, the insulating tape of invention example 9 was molded to have a thickness of 0.3mm and a length and width of 50mm, and the electric field magnification was determined. The "electric field multiplication factor" obtained here is preferably small in the amount of space charge accumulated, and therefore is preferably small, and more preferably 130% or less. The results are shown in tables 1 and 2.
[ Table 2]
Regarding the type of screw, "F" means that no resin mixing portion is provided, and "M" means that a Madoc-type resin mixing portion is provided.
Underlining in the table indicates the case outside the appropriate range of the present invention and the case where the evaluation results did not reach the acceptable level in the examples of the present invention.
From the evaluation results in tables 1 and 2, it was confirmed that the evaluation sheets, insulating tapes and insulating layers of examples 1 to 8 of the present invention, which contain at least a modified polyolefin resin modified with a specific molecule having a polar group, an unmodified polyolefin resin and an antioxidant and have a sea-island structure in which the average diameter of the island phase is within the suitable range of the present invention, have an electric field expansion ratio of 130% or less.
From the above results, it was confirmed that the evaluation sheets, the insulating tapes and the insulating layers of examples 1 to 8 of the present invention hardly cause dielectric breakdown.
On the other hand, the evaluation sheet of comparative example 1 had no sea-island structure, and therefore had a high electric field magnification and did not satisfy the acceptable level.
In the evaluation sheets of comparative examples 2 to 3, the insulating tape of comparative example 4, and the insulating layer of the covered connection portion of the power cable of comparative example 5, the average diameter of the island phase in the sea-island structure was large, i.e., larger than 2 μm, and therefore the electric field gain ratio was high and did not satisfy the acceptable level.
Description of the reference numerals
1 insulating resin composition
11 the first phase (sea phase)
12 second phase (island phase)
2. 3, 30a, 30b power cable
21. 31a, 31b conductor
22. 32a, 32b inner conductor layer
23. 33a, 33b insulating layer
24. 34a, 34b outer semiconducting layer
25. 35a, 35b metal shielding layer
26. 36a, 36b sheaths
20. 370 composite coating film
37 connecting structure part
371 connecting part
372 inner semiconductive layer
373 insulating layer
374 outer semiconducting layer
4. 5 screw rod
41. 51 to the installation in the extruder
42. 52 full-thread screw
43 resin mixing section
Length of exposed conductor of E1, E2 power cable
Diameter of D screw
Length of L-shaped screw
Claims (12)
1. An insulating resin composition comprising at least a base resin and an antioxidant, wherein the base resin comprises a modified polyolefin resin modified with a molecule having a polar group and an unmodified polyolefin resin,
the modified polyolefin resin is modified with at least 1 selected from the group consisting of an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative as a molecule having a polar group,
the base resin has a so-called sea-island structure in which a second phase containing the modified polyolefin resin is present in a first phase containing the unmodified polyolefin resin, and the second phase has an average diameter of 2 μm or less.
2. An insulating tape for forming an insulating layer of a power cable, which is produced from the insulating resin composition according to claim 1,
the thickness of the tape is in the range of 30 μm to 250 μm, and the width of the tape is in the range of 3mm to 40 mm.
3. A power cable having:
a conductor; and
a composite coating film comprising an inner semiconductive layer made of a first conductive resin, an insulating layer, and an outer semiconductive layer made of a second conductive resin, which are laminated in this order on the outer periphery of the conductor, wherein the insulating layer is formed by using the insulating resin composition according to claim 1 as a raw material and crosslinking at least the modified polyolefin resin in the second phase and at least the unmodified polyolefin resin in the first phase.
4. A power cable including a connection structure portion, the connection structure portion including:
a connecting section in which the exposed ends of the conductors of the plurality of power cables are conductor-connected to each other; and
a composite coating film comprising an inner semiconductive layer made of a first conductive resin, an insulating layer, and an outer semiconductive layer made of a second conductive resin, which are laminated in this order on the outer periphery of the connecting portion, wherein the insulating layer is formed by using the insulating resin composition according to claim 1 as a raw material and crosslinking at least the modified polyolefin resin in the second phase and at least the unmodified polyolefin resin in the first phase.
5. The power cable according to claim 4, wherein the insulating layer is formed by winding and crosslinking an insulating tape for forming an insulating layer having a tape thickness in a range of 30 μm or more and 250 μm or less and a tape width in a range of 3mm or more and 40mm or less around the outer periphery of the inner semiconductive layer.
6. A power cable according to any one of claims 3 to 5, wherein the total thickness of the inner and outer semiconductive layers is 5mm or less.
7. A method for producing an insulating resin composition, comprising the steps of:
an unmodified polyolefin resin and an antioxidant are added to a modified polyolefin resin modified with at least 1 selected from an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative which are molecules having a polar group, and then kneaded to obtain a base resin in which the modified polyolefin resin is diluted with the unmodified polyolefin resin, and the base resin has a so-called sea-island structure in which a second phase containing the modified polyolefin resin is present in a first phase containing the unmodified polyolefin resin, and the second phase has an average diameter of 2 [ mu ] m or less.
8. A method for producing an insulating resin composition, comprising the steps of:
a method for producing a polyolefin resin composition, which comprises adding an unmodified polyolefin resin and an antioxidant to a modified polyolefin resin modified with at least 1 selected from an unsaturated dicarboxylic acid, an unsaturated dicarboxylic anhydride and an unsaturated dicarboxylic anhydride derivative which are molecules having a polar group, to prepare a diluted polyolefin pellet comprising a base resin in which the modified polyolefin resin is diluted with the unmodified polyolefin resin, adding a crosslinking agent to the prepared diluted polyolefin pellet, and dry-blending the pellets so that the base resin has a so-called sea-island structure in which a second phase comprising the modified polyolefin resin is present in a first phase comprising the unmodified polyolefin resin and the second phase has an average diameter of 2 [ mu ] m or less.
9. A method for manufacturing an insulating tape for forming an insulating layer of a power cable, the method comprising:
a step of forming a film by extrusion molding the insulating resin composition according to claim 1, and cooling the surface temperature of the film to the melting point of the unmodified polyolefin resin or less within 15 seconds after the insulating resin composition is extruded; and
and a step of slitting the film to form a tape.
10. A method for forming an insulating layer on the outer surface of a connecting portion of a power cable, comprising the steps of:
an insulating layer is formed on the outer surface of a connection part formed by connecting conductors of a plurality of power cables with exposed ends of the conductors by using the insulating resin composition according to claim 1,
and subjecting the connecting portion on which the insulating layer is formed to a pressure-heating treatment under conditions of 300kPa to 1000kPa inclusive and 140 ℃ to 280 ℃ inclusive, thereby crosslinking an unmodified polyolefin resin and a modified polyolefin resin of the base resin contained in the insulating layer.
11. The method of forming an insulating layer according to claim 10, wherein the insulating layer is formed on the outer periphery of the connecting portion by winding an insulating tape for forming an insulating layer, the insulating tape being made of the insulating resin composition, having a tape thickness of 30 μm or more and 250 μm or less and a tape width of 3mm or more and 40mm or less.
12. A method for manufacturing a power cable, comprising a step of laminating an inner semiconductive layer, an insulating layer and an outer semiconductive layer in this order on the outer periphery of a conductor, and crosslinking at least the insulating layer,
the insulating layer is laminated by extruding the insulating resin composition according to claim 1 onto the outer periphery of the inner semiconductive layer,
cooling the surface temperature of the laminated insulating layer to the melting point of the unmodified polyolefin resin or less within 15 seconds after being extruded to the outer periphery of the inner semiconductive layer,
the crosslinking step of the insulating layer is performed by: and subjecting the insulating layer to a pressure-heating treatment under conditions of 300kPa to 1000kPa inclusive and 140 ℃ to 280 ℃ inclusive, thereby crosslinking the unmodified polyolefin resin and the modified polyolefin resin of the base resin contained in the insulating layer.
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| JP2019069322 | 2019-03-29 | ||
| JP2019-069322 | 2019-03-29 | ||
| PCT/JP2020/014712 WO2020204012A1 (en) | 2019-03-29 | 2020-03-30 | Insulating resin composition and production method therefor, insulating tape and production method therefor, insulating layer formation method, and power cable and production method therefor |
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| US (1) | US11990253B2 (en) |
| EP (1) | EP3950821A4 (en) |
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| CN116769359A (en) * | 2022-03-09 | 2023-09-19 | 昭和电线电缆株式会社 | Semiconductive coating, preparation method thereof and terminal treatment method of power cable |
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| WO2024117047A1 (en) * | 2022-11-30 | 2024-06-06 | 住友化学株式会社 | Recycled material, film, sheet and method for producing recycled material |
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| WO2018030160A1 (en) * | 2016-08-09 | 2018-02-15 | 株式会社Ｎｕｃ | Insulating resin composition for direct-current power cable, crosslinked resin, direct-current power cable, member for forming insulating reinforcement layer of direct-current power cable junction, and direct-current power cable junction |
| JP2019011448A (en) * | 2017-06-30 | 2019-01-24 | 日立金属株式会社 | cable |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116769359A (en) * | 2022-03-09 | 2023-09-19 | 昭和电线电缆株式会社 | Semiconductive coating, preparation method thereof and terminal treatment method of power cable |
| CN115312271A (en) * | 2022-06-28 | 2022-11-08 | 江苏上上电缆集团有限公司 | Three-layer co-extrusion production method of medium-voltage polypropylene insulated wire core |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3950821A4 (en) | 2022-12-28 |
| CN113597447B (en) | 2024-03-05 |
| JP6852229B2 (en) | 2021-03-31 |
| KR102695316B1 (en) | 2024-08-13 |
| US11990253B2 (en) | 2024-05-21 |
| WO2020204012A1 (en) | 2020-10-08 |
| KR20210144724A (en) | 2021-11-30 |
| US20220157488A1 (en) | 2022-05-19 |
| EP3950821A1 (en) | 2022-02-09 |
| JPWO2020204012A1 (en) | 2021-04-30 |
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